Trifluoroacetic acid methylene chloride → Phenylmethyl N-(1,4,5,6-tetrahydropyrrolo[3,4-c]pyrazol-3-yl)carbamate

HRID 2353428Notes

Reaction equation

HRID 2353428 reaction equation
[CH2:1]([O:8][C:9]([NH:11][C:12]1[C:13]2[CH2:19][N:18](C(OC(C)(C)C)=O)[CH2:17][C:14]=2[NH:15][N:16]=1)=[O:10])[C:2]1[CH:7]=[CH:6][CH:5]=[CH:4][CH:3]=1.ClCCl.FC(F)(F)C(O)=O>>[NH:15]1[C:14]2[CH2:17][NH:18][CH2:19][C:13]=2[C:12]([NH:11][C:9](=[O:10])[O:8][CH2:1][C:2]2[CH:3]=[CH:4][CH:5]=[CH:6][CH:7]=2)=[N:16]1

Participants

3

Reactant 2

HCID 21863450Trifluoroacetic acid methylene chlorideHCID 86635438HCID 86635438, compound

Product 1

HCID 57931357Phenylmethyl N-(1,4,5,6-tetrahydropyrrolo[3,4-c]pyrazol-3-yl)carbamate

Procedure

To the product from Step B was added 4 mL of 1:1 dichloromethane/trifluoroacetic acid, and the solution was stirred for 60 min then concentrated in vacuo. The crude oil was purified by preparative thin layer chromatography using an Analtech® 1500 micron plate (10% methanol/ethyl acetate, 1% concentrated ammonium hydroxide) to give the title compound as a white solid. LC/MS 259.2 (M+1).

Workup

  1. concentrationthen concentrated in vacuo
  2. customThe crude oil was purified by preparative thin layer chromatography

Sources & evidence

ORD record
ord-9d994f815ecf47d9bd16ea9a9e361dc2
Source dataset
uspto-grants-2010_07
Patent number
US07750034B2

Reaction notes

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